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土壤中六六六和滴滴涕定量检测的一种快捷方法

         

摘要

本文改进土壤中六六六、滴滴涕测定国标方法(GB/T 14550-2003),建立了石油醚/丙酮(1/1, v/v)混合溶剂萃取,超声波提取,浓硫酸净化,毛细管气相色谱法(电子捕获检测器)定量检测土壤中有机氯的方法.方法对目标物γ-六六六、o,p'-DDT、p,p'-DDT的检出限为0.01-0.04μg/kg,对4种供试砖红壤土样的加标回收率达到81.24%~102.36%,相对标准偏差为0.42%~3.5%.该方法在无索氏提取器和固相萃取装置实验条件下使用,具可批量处理,溶剂无毒/用量少,提取时间短和易操作优点.%  A simple and fast improved GB/T 14550-2003 analytical method was developed for the quantitative determination of HCH and DDT residues in lateritic paddy soil samples. The analytes were extracted from the soil samples by means of ultrasound-assisted extraction,using the acetone and petroleum ether mixed solvent(1/1, v/v)as extractants,and the extract was purified with concentrated sulfuric acid. Separation and determination were made by using capillary column gas chromatography with micro-electron capture detector(μECD). Recoveries of 80.96-83.45%,82.29-86.15%, and 100-102.36%,respectively,have been obtained forγ-HCH, o,p’-DDT and p,p’-DDT in blank samples spiked at the level of 1.0 mg/kg,with RSD of 0.42%to 3.5%. The detection limits for the analytes were in the range of 0.01-0.04μg/kg. The proposed method was conducted when no soxhlet extraction was applied,using less solvent and taking significantly less time than GB/T 14550-2003 method.

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